Toothpaste Composition

ABSTRACT

A toothpaste composition includes a structurant and a thickener, wherein the toothpaste composition has a predetermined viscosity and phase angle by using the structurant instead of reducing the content of a thickener, and thereby has an improved release property during use while maintaining a shape retention property of the toothpaste, and has an improved feeling of refreshment, flavor releasing power, cleaning power, and stain removal power. Further, provided is a toothpaste composition including a chelating agent containing phosphate and silica, wherein the chelating agent is supersaturated to precipitate phosphate to provide strong cleaning power, a whitening effect, a stain removal effect, and a crunchy sensation. Further, provided is a toothpaste composition including a peroxide, a thickener, and a spreading agent, wherein the peroxide and the thickener are separated from each other, providing excellent sense of use, stability, and a whitening effect in an anhydrous state.

CROSS-REFERENCE TO RELATED APPLICATIONS

The present application is a divisional of U.S. application Ser. No.17/053,974, filed Nov. 9, 2020 which is a national phase entry under 35U.S.C. § 371 of International Application No. PCT/KR2020/004266, filedMar. 27, 2020, which claims priority to Korean Patent Application Nos.10-2019-0036188, 10-2019-0036187 and 10-2019-0036186 filed Mar. 28,2019, all the disclosures of which are incorporated herein by reference.

TECHNICAL FIELD

The present invention relates to a toothpaste composition including astructurant and a thickener, and specifically, a toothpaste compositionhaving an improved shape retention property, release property when used,feeling of refreshment, flavor releasing power, cleaning power, andstain-removing power.

Further, the present invention relates to a toothpaste compositionhaving an improved whitening effect and sense of use, specifically, atoothpaste composition including silica and a chelating agent containingphosphate, wherein the chelating agent is supersaturated to precipitatephosphate, and particles of the precipitated phosphate realize a strongcleaning power, a whitening effect, stain removal, and a crunchysensation when used.

Further, the present invention relates to a toothpaste compositionincluding a peroxide, a thickener, and a spreading agent, wherein theperoxide and the thickener are separated from each other, andspecifically, a toothpaste composition having excellent sense of use,stability, and a whitening effect even in an anhydrous state.

BACKGROUND ART

A release property of toothpastes is important at the time of use forrapid delivery of active ingredients. An excellent release property hasa great influence on the rapid delivery of the active ingredientssupported in the toothpaste, foam generation, and consumers' sense ofuse.

In addition, existing common toothpastes are blended with xanthan gum,etc. to prepare a thickening system, so that the toothpaste is allowedto be discharged from a container such as a tube. In other words, athickener or a binder is included to build viscosity of the toothpaste.In existing toothpaste compositions, the thickener or the binder isincluded at a high concentration.

However, when the thickening force is strong, the thickener creates abinding force between the components throughout the toothpaste, and thiscauses a problem in that the toothpaste stuck together is not easilyreleased by saliva or tooth brushing. For this reason, liquid toothpastecompositions have been developed. However, liquid toothpastecompositions have a disadvantage of easily flowing away due to lowviscosity, and thus are widely used as mouthwashes that performfunctions of inhibiting oral bacteria and removing bad breath. However,due to the lack of cleaning ingredients and easy flowing, they do notexert sufficient brushing effects such as removal of plaque and removalof oral bacteria in the mouth (Korean Patent Application No.2001-7004081).

With the growing interest in tooth whitening, there are many kinds ofwhitening toothpastes on the market. However, even though thetoothpastes include an effective whitening agent, the toothpastes areused for a short time of 1 minute to 3 minutes, and thus it is necessaryin terms of sense of use and effect to rapidly release the activeingredient or flavor. For the tooth whitening, staining materials on thetooth surface or staining materials between the teeth must be removed.

Discoloration on the tooth surface is known to result from deposition offood-derived pigments (tea, coffee, red wine, etc.) as extrinsic stains,discoloration due to Maillard reaction by denaturation of glycoproteinsin the saliva covering the dental surface, discoloration bysulfur-containing amino acids or metals, or discoloration of double bondmoieties in proteins.

However, although toothpastes containing particles have been developedin order to provide strong cleaning power and a feeling of cleaning,problems of unsatisfactory effects, safety, and environmental pollutionhave been raised.

Further, since a toothpaste has a foaming agent, an abrasive, and anactive ingredient, it has basic properties of providing cleaning powerand a feeling of refreshment when used with a toothbrush. However,except for chemical bleaching by hydrogen peroxide, discoloration on thetooth surface is difficult to remove.

Generally, consumers want to receive whitening effects only with theirdaily brushing for their convenience. Whitening toothpastes should beable to break double bonds of staining materials by penetrating thewhitening component to the dentin. A substance having this effect isperoxide, which has a low molecular weight and is decomposed into waterand oxygen.

However, hydrogen peroxide is highly reactive with water, and thus it iseasily decomposed in water and has poor compatibility with othercomponents of toothpastes such as polymers, abrasives, fluoride, foamingagents, etc. In particular, toothpastes containing hydrogen peroxidehave a disadvantage in that an abrasive cannot be added togethertherewith, and therefore, it is difficult to achieve a synergisticeffect of two mechanisms in the whitening effect. For this reason,toothpastes containing water as a solvent and a large amount of hydrogenperoxide while having high viscosity suitable for tube toothpaste,fluoride, a foaming agent, an abrasive, a flavor, etc. have poorstability of peroxide at a high temperature over time, and as a result,phase separation of hydrogen peroxide occurs, and thus itscommercialization is difficult.

DISCLOSURE Technical Problem

There have been many efforts to solve the problems of the conventionalart, and as a result, the present inventors found that when astructurant is used instead of reducing the content of a thickener, atoothpaste composition has an improved release property during use whilemaintaining a shape retention property by having a predeterminedviscosity and phase angle, and the toothpaste composition has excellentcleaning power and stain-removing power, thereby completing thetoothpaste composition of the present invention.

The present inventors also found that when a toothpaste compositionincludes a chelating agent with phosphate supersaturation, thetoothpaste composition may have strong cleaning power, a whiteningeffect, an excellent stain removal effect, and a crunchy sensation whenused due to the precipitated phosphate particles, thereby completing thetoothpaste composition of the present invention.

The present inventors also found that when a toothpaste compositionincludes a peroxide, a thickener, and a spreading agent, wherein theperoxide and the thickener are separated from each other, it may haveexcellent sense of use and a whitening effect in spite of using afoaming agent, an abrasive, etc. having high compatibility with hydrogenperoxide in an anhydrous base, thereby completing the toothpastecomposition of the present invention.

Technical Solution

An object of the present invention is to provide a toothpastecomposition including a structurant and a thickener.

Another object of the present invention is to provide a toothpastecomposition including silica and a chelating agent containing phosphate,wherein the chelating agent is supersaturated to precipitate phosphate,and the amount of the precipitated phosphate is 2% to 10% based on thetotal weight of the toothpaste composition.

Still another object of the present invention is to provide a toothpastecomposition including a peroxide, a thickener, and a spreading agent.

Still another object of the present invention is to provide a toothpastecomposition including a peroxide and a thickener, wherein the peroxideand the thickener are separated from each other.

Advantageous Effects

The toothpaste composition according to the present invention has apredetermined viscosity and phase angle by using a structurant insteadof reducing the content of a thickener, and thereby has an improvedrelease property during use while maintaining a shape retention propertyof the toothpaste, as well as excellent cleaning power and stain removalpower.

Further, the toothpaste composition according to the present inventionincludes a chelating agent with phosphate supersaturation, and therebyhas a crunchy sensation due to the supersaturated and precipitatedphosphate particles, as well as strong cleaning power, an excellentwhitening effect, and a stain removal effect.

Further, the toothpaste composition according to the present inventionincludes a peroxide, a thickener, and a spreading agent, in which theperoxide and the thickener are separated from each other, and therebyhas an excellent whitening effect due to more rapid decomposition ofhydrogen peroxide in an anhydrous state even though a foaming agent, anabrasive, etc. having high compatibility with hydrogen peroxide areused, and also has excellent sense of use and stability.

BRIEF DESCRIPTION OF DRAWINGS

FIG. 1 shows a value of loss tangent (tan δ) indicating a ratio ofviscosity to elasticity (energy loss/energy stored).

FIG. 2 shows classification of physical properties according to thephase angle.

FIG. 3 shows a comparison of toothpaste tubes cut in half after thetoothpaste in the tube was stored for 4 weeks in a 50° C. incubator.

BEST MODE FOR CARRYING OUT THE INVENTION

Hereinafter, the present invention will be described in more detail.

Meanwhile, each description and embodiment disclosed in this disclosuremay also be applied to other descriptions and embodiments. That is, allcombinations of various elements disclosed in this disclosure fallwithin the scope of the present invention. Further, the scope of thepresent invention is not limited by the specific description below.

Further, those skilled in the art will recognize, or will be able toascertain using no more than routine experimentation, many equivalentsto the specific embodiments of the invention described herein. Further,these equivalents should be interpreted to fall within the presentinvention.

To solve the above problems, an aspect of the present invention providesa toothpaste composition including a structurant and a thickener.

As used herein, the term “structurant” means a material that aggregatestoothpaste components by a polymer network due to strong interactionbetween polymers themselves, and has high gelation ability butrelatively low interaction with other toothpaste components includingwater, such that its structure is easily collapsed by saliva, wettoothpaste before use, or an external force such as brushing, etc., andas a result, its release property is strengthened. The structurant is tomake up for disadvantages of using the thickener, and it may be includedto improve the release property and to maintain the shape retentionproperty, instead of the thickener.

The structurant of the present invention may be one or more componentsselected from the group consisting of carrageenan and carbomer, but isnot limited thereto.

As used herein, the term “phase angle” refers to an angle correspondingto a tangent value of a trigonometric function for‘viscosity/elasticity’, and is specifically as follows.

In a dynamic oscillatory shear test, ω represents oscillation frequency,δ represents a phase lag between stress and strain, G′ (an elasticmodulus with no energy loss due to no phase lag between stress andstrain) represents an elastic component of a material and is a measureof the stored energy, and G″ represents viscosity of the material and isa measure of the energy lost as heat. In particular, G″/G′, a ratio ofG″ to G′, is called loss tangent (tan δ), indicating a ratio ofviscosity to elasticity of the material (energy loss/energy stored),which is also called phase angle (FIG. 1 ).

A solid is in a state of a low release property, and a liquid is in astate of a high release property. From the concept of phase angle, anideal solid refers to a perfectly elastic body, and its deformation isstored as energy. In other words, compared to elasticity (a recoveryforce to return to its original shape when an external force isapplied), viscosity (a degree of content flowing when an external forceis applied) is very low, and the phase angle is close to 0. Conversely,an ideal liquid refers to a perfectly viscous body, and its deformationis not stored as energy but lost. In other words, its elasticity is verylow compared to its viscosity, and the phase angle approaches 90 degrees(FIG. 2 ).

The toothpaste composition of the present invention may have a phaseangle of 20 to 90, specifically, 25 to 70, 30 to 50, or 30 to 40, andmore specifically, 20 to 50, 20 to 40, or 20 to 30, but is not limitedthereto. In particular, the toothpaste of the present invention isrelatively close to a liquid state compared to conventional toothpastes.Due to this state, the toothpaste of the present invention has a veryexcellent release property. However, when the toothpaste is too close tothe liquid state, it is difficult to discharge a desired amount of thetoothpaste onto a toothbrush, and the shape retention property of thetoothpaste when it is on a toothbrush becomes problematic. Therefore, itis preferable that the toothpaste have a predetermined level of phaseangle.

As used herein, the term “viscosity” refers to a fluid's internalresistance. In the present invention, the viscosity represents viscosityof the toothpaste itself measured at room temperature, which is theresult of measuring viscosity using a viscometer (Brookfield RVF) and aspindle bar of #7 at a rotational speed of 20 rpm.

As used herein, the term “low-shear viscosity” refers to shear viscositymeasured at a low shear rate, which means how hard the state of a liquidin a solid is, and specifically means how well it withstands the statewhen an external force is applied. In the present invention, thelow-shear viscosity is defined as viscosity at a shear rate of 0.1 s⁻¹.The low-shear viscosity may be easily measured using a rheometer.

The toothpaste composition may have a viscosity of 60,000 cP to 150,000cP.

In a specific embodiment, the toothpaste composition of the presentinvention, which includes a peroxide, a thickener, and a spreadingagent, may have a viscosity of 60,000 cP to 150,000 cP, specifically70,000 cP to 150,000 cP, or more preferably 80,000 cP to 150,000 cP, andmore specifically 90,000 cP to 150,000 cP even in an anhydrous base, butis not limited thereto. Depending on the viscosity, the toothpastecomposition of the present invention has excellent sense of use, such asfeelings of refreshment and cleaning, foam generation, flavor releasingpower, etc.

In another specific embodiment, the toothpaste composition of thepresent invention, which includes silica and a chelating agentcontaining phosphate, may have a viscosity of 60,000 cP to 110,000 cP.Specifically, the toothpaste may exhibit the above viscosity by usingcarrageenan, xanthan gum, and thickening silica, but is not limitedthereto. Owing to the above viscosity, dispersion of the abrasive andsupersaturated phosphate may be stably achieved.

In still another specific embodiment, the toothpaste composition of thepresent invention, which includes a structurant and a thickener, mayhave a viscosity of 50,000 cP to 110,000 cP, specifically, 50,000 cP to100,000 cP, even after being stored at 20° C. to 30° C. for 7 days, butis not limited thereto.

In the case of existing common toothpaste compositions, a toothpastecomposition having a final viscosity of 40,000 cP or less, morespecifically 20,000 cP or less was confirmed to have a very excellentrelease property, while a toothpaste composition having a viscosity of50,000 cP or more was confirmed to have a very low release property. Thetoothpaste composition having a viscosity of 50,000 cP or more wasconfirmed to be suitable for a tube formulation as a paste formulation.

Unlike this toothpaste composition, the toothpaste composition of thepresent invention was confirmed to have a very excellent releaseproperty, even though its viscosity is 50,000 cP or more.

As used herein, the term “thickener” refers to a material that acts, asa binder in the toothpaste composition, to prevent the solid powdercomponent from being separated from the liquid component. In addition tothe function of preventing separation of toothpaste components, thethickener affects an appearance of the toothpaste, such as its shaperetention property, transparency, etc., extrudability from a toothpastetube, and properties when used, such as its release property duringbrushing, etc., and also affects efficacy and effects such as drugdelivery, etc.

The thickener may be any type of polymer as long as it is awater-soluble polymer, and the thickener may consist of an organicthickener and an inorganic thickener.

The thickener of the present invention may be specifically one or morecomponents selected from the group consisting of polyvinyl pyrrolidone(PVP), crosslinked PVP, polyvinyl alcohol (PVA), carboxymethyl cellulose(CMC), polyethylene glycol (PEG), carboxypolymethylene, carboxypropylcellulose, poloxamer, carrageenan, carboxyvinyl polymers, xanthan gum,and polyvinyl pyrrolidone/vinyl acetate copolymers, and morespecifically, it may be PVP or crosslinked PVP, but is not limitedthereto.

The thickener of the toothpaste composition of the present invention maybe an organic thickener or an inorganic thickener.

In the present invention, the “organic thickener” may specifically referto a material that has a characteristic of a relatively high interactionwith water, as compared with an interaction between organic thickeners.Due to this characteristic, the organic thickener may increase athickening power of the toothpaste composition.

A content ratio of the structurant and the organic thickener of thepresent invention may be 0.2:1 to 6:1, specifically 0.3:1 to 5:1, andmore specifically 0.5:1 to 4:1, but is not limited thereto.

The organic thickener of the present invention may be specifically oneor more components selected from the group consisting of poloxamer,carbomer, polysaccharide, and carboxymethyl cellulose (CMC), and morespecifically, one or more components selected from the group consistingof poloxamer, carbomer, and polysaccharide, but is not limited thereto.

The polysaccharide may be one or more components selected from the groupconsisting of xanthan gum, gellan gum, and locust bean gum, but is notlimited thereto.

The inorganic thickener of the present invention may be one or morecomponents selected from the group consisting of thickening silica,colloidal silica, and fumed silica, but is not limited thereto.

However, among the organic thickeners, carboxymethyl cellulose (CMC) isknown to have side effects such as gastrointestinal disorders,constipation, diarrhea, etc., when excessively ingested. In this regard,the toothpaste composition according to an aspect of the presentinvention, which includes the structurant and the thickener, may notinclude carboxymethyl cellulose (CMC) in one exemplary embodiment, butis not limited thereto.

In particular, CMC has a characteristic that its hydration anddispersion do not occur well under conditions of low water content.Unlike the common toothpaste compositions with high water content, thetoothpaste composition of the present invention with low water contentis characterized by having a relatively high content of the inorganicthickener, instead of reducing the content of CMC.

In one exemplary embodiment of the present invention, the organicthickener may be included in an amount of 0.0001% to 2%, specifically0.0001% to 1%, and more specifically 0.0001% to 0.6%, based on the totalweight of the toothpaste composition, but is not limited thereto.

In the present invention, the inorganic thickener may be specificallyone or more components selected from the group consisting of thickeningsilica, colloidal silica, and fumed silica, but is not limited thereto.The inorganic thickener is a component that does not greatly influencethe release property, and exhibits sufficient viscosity even at lowwater content.

In one exemplary embodiment of the present invention, the inorganicthickener may be included in an amount of 1% to 30%, specifically 1.5%to 20%, and more specifically 2% to 10%, based on the total weight ofthe toothpaste composition, but is not limited thereto.

The toothpaste composition of the present invention may include water orno water.

This may vary depending on the composition of the toothpastecomposition.

The toothpaste composition of the present invention may further includewater in an amount of 15% by weight or less, 10% by weight or less, 1%by weight to 15% by weight, 1% by weight to 10% by weight, or 0.01% byweight to 10% by weight, specifically 1% by weight to 8% by weight, 1%by weight to 7% by weight, 0.01% by weight to 8% by weight, 0.01% byweight to 6% by weight, or 0.01% by weight to 5% by weight, and morespecifically 2% by weight to 6% by weight, 0.01% by weight to 3% byweight, or 0.01% by weight to 2% by weight, based on the total weight ofthe toothpaste composition, but is not limited thereto.

In the case of not containing water or containing a small amount water,liquid polyols such as glycerin, PEG, PG, etc. may be included as adispersion solvent of the toothpaste components, but are not limitedthereto. Specifically, the liquid polyol may be included as a dispersionsolvent of the toothpaste composition according to the presentinvention, as long as it does not cause a substantial increase in theviscosity of the composition by interaction with the thickener. In thiscase, the liquid polyol may be included in an amount of 20% to 80% basedon the total weight of the composition, but is not limited thereto.

In particular, the liquid polyol may include glycerin, and in thisregard, the glycerin may be included in an amount of 30% to 70%,specifically 40% to 70%, and more specifically 50% to 70%, based on thetotal weight of the composition, but is not limited thereto.

In general, when toothpaste compositions have high water content, theviscosity may be increased and the binding of the toothpaste basecomponents may be strengthened due to the thickener, and as a result,the release property is weakened.

Accordingly, in order to maintain the shape retention property even whenthe water content is reduced, the present invention is characterized byincluding the structurant and the inorganic thickener, instead ofreducing the content of the organic thickener, and thereby has excellentshape retention and release properties.

According to one exemplary embodiment of the present invention, it wasconfirmed that the toothpaste composition of the present invention haseffects of improving the shape retention property and the releaseproperty.

As used herein, the term “shape retention property” refers to a propertyof maintaining the original shape of the toothpaste without it flowingdown on a toothbrush when used by discharging the toothpaste on thetoothbrush head. As the shape retention property is higher, a user'semotional satisfaction becomes higher.

However, when the thickening force is increased in order to improve theshape retention property, a bonding force between the components iscreated throughout the toothpaste due to the thickener, which may causea problem in that a lump of toothpaste is not well released by saliva ortooth brushing.

Accordingly, the toothpaste composition of the present invention ischaracterized by having an excellent release property and an improvedshape retention property at the same time.

As used herein, the term “release property” refers to dispersibilitywhereby a lump of toothpaste is released when it gets wet due to salivaor water after being discharged from a container containing thetoothpaste to a toothbrush. Such excellent release property has a greatinfluence on the rapid delivery of the medicinal ingredients supportedin the toothpaste, foam generation, and consumers' sense of use.

As the toothpaste is more rapidly dispersed in water, it is more rapidlydispersed in the mouth, and this rapid dispersibility is an importantfactor in increasing the contact time of an anti-cavity ingredient withthe tooth surface. In the present invention, it was confirmed that therapid dispersibility is mainly related to the gel structure andthixotropy, and it was found that the thickening silica having a highoil absorption value has a great influence on the dispersibility.However, it was not easy to achieve excellent rheology while showing aviscosity of 50,000 cP or more only by thickening silica alone.Accordingly, it was confirmed that when the water content and theconcentration of the thickener in the toothpaste are reduced, anexcellent release property may be achieved even in the toothpastecomposition having a viscosity suitable for being put in a tube as apaste formulation. In addition, it was confirmed that the sense of useand cleaning effect were also excellent due to the rapid release offlavor and active ingredients.

According to one exemplary embodiment of the present invention, it wasconfirmed that the toothpaste composition of the present invention haseffects of improving a feeling of refreshment and flavor releasingpower.

It was also confirmed that the toothpaste composition of the presentinvention has an excellent release property, and thereby has theexcellent flavor releasing power and the improved feeling ofrefreshment.

According to one exemplary embodiment of the present invention, it wasconfirmed that the toothpaste composition of the present invention haseffects of improving cleaning power and stain removal power.

It was also confirmed that the toothpaste composition of the presentinvention has an excellent release property, and thereby has excellenteffects of removing stains on the tooth surface and brightening teeth.

The toothpaste composition of the present invention, which includes thestructurant and the thickener, may further include one or morecomponents selected from the group consisting of an abrasive, asurfactant, a humectant, a medicinal agent, an additive, and a foamingagent, but is not limited thereto.

As used herein, the term “abrasive” refers to a material that serves toremove dental plaque by polishing the surface of the tooth.

The abrasive of the present invention may be one or more selected fromthe group consisting of calcium pyrophosphate (CPP), calcium carbonate,insoluble sodium metaphosphate, zirconium silicate, hydroxyapatite,dental type silica, precipitated silica, hydrated alumina, silica gel,and dicalcium phosphate dehydrate (DCPD).

As used herein, the term “surfactant” refers to an agent that improvescompatibility and cleansing effect of an oral composition and acts toquickly disperse and penetrate the medicinal ingredients to easilyremove foreign substances in the mouth.

In the present invention, the surfactant may be an anionic surfactantand a non-ionic surfactant alone or in a mixture thereof. Preferably,the surfactant may be one or more selected from the group consisting ofone or more anionic surfactants selected from the group consisting ofsodium lauryl sulfate and sodium alkylsulfate; and one or more non-ionicsurfactants selected from the group consisting of copolymers ofpolyoxyethylene and polyoxypropylene, polyoxyethylene sorbitan fattyacid, alkanolamide fatty acid ester, sucrose fatty acid ester,polyoxyethylene sorbitan fatty acid ester, polyoxyethylene fatty acidester, polyoxyethylene castor oil derivatives, N-lauryl sarcosinate,sodium lauryl ether sulfate, polysorbate, decaglycerin monolaurate,sorbitan monooleate, alkyl polyglucoside, and cocoamide DEA.

As used herein, the term “humectant” refers to a substance that, as anessential base component for preparing ointment formulations, plays arole in preventing drying and solidification when the oral compositionis exposed to air, providing gloss for the surface of the toothpaste,and also providing a sweetening effect during tooth brushing dependingon the type.

In the present invention, the humectant may be one or more selected fromthe group consisting of a sorbitol solution, glycerin, polyethyleneglycol, and propylene glycol.

As used herein, the term “medicinal agent” refers to a substance thatmay exhibit various medicinal effects for teeth cleansing and cleaning,and includes various functional ingredients and herbal materials thatmay be included in a toothpaste. Specifically, it may include a fluoridethat forms a fluoride film on teeth and makes teeth resistant to an acid(lactic acid, etc.), which is a metabolite of caries bacteria.

As used herein, the term “foaming agent” refers to one that improves thesense of use of a product, helps the cleaning action, acceleratesdispersion and penetration of other medicinal ingredients, and reducesthe interfacial tension to easily remove foreign substances from themouth.

As used herein, the term “additive” may refer to a flavoring agent, asweetening agent, a pH adjusting agent, a brightening agent, anexcipient, a preservative, and a coloring agent, and the content thereofis within the usual range.

The flavoring agent is edible, and synthetic flavoring agents (e.g.,menthol, a green tea flavor, a mint flavor, etc.), extracts extractedfrom plants (e.g., peppermint oil, spearmint oil, sage oil, eucalyptol,eugenol, etc.), or extracts extracted from fruits may be used.

Sodium saccharin, xylitol, etc. may be most commonly used as thesweetening agent; sodium hydrogen carbonate, etc. may be used as the pHadjuster; and titanium oxide may be used as the brightening agent. Inaddition, hydroxyapatite may be used as the excipient, and food coloringis mainly used as the coloring agent.

The preservative is used to prevent microbial contamination that mayoccur during preparation and use of oral compositions and to helpprolong the preservation of toothpastes. Sodium benzoate or parabens maybe used as the preservative.

Still another aspect of the present invention provides a toothpastecomposition including silica and a chelating agent containing phosphate,wherein the chelating agent is supersaturated to precipitate phosphateand the content of the precipitated phosphate is 2% or more, andspecifically 2% to 10%, based on the total weight of the toothpastecomposition.

The “precipitated phosphate” of the present invention refers tophosphate added to the composition in a maximum dissolution amount ormore with respect to a solvent, particularly, water at 25° C., and whenthe solvent is water, the water content may be determined by a method ofmeasuring water contents commonly known in the art, for example, theKarl Fischer method.

As used herein, the term “chelating agent” refers to a compositionincluding a metal phosphate. Specifically, the chelating agent may beone or more components selected from the group consisting of tetrasodiumpyrophosphate (TSPP), sodium acid pyrophosphate (SAPP), and sodiumhexametaphosphate (SHMP), and more specifically may be SHMP, but is notlimited thereto.

The chelating agent of the present invention is supersaturated toprecipitate phosphate. The precipitated phosphate has particles, and dueto these particles, the toothpaste composition of the present inventionmay realize a crunchy sensation of use, and may exhibit improvedcleaning power and a whitening effect.

In the present invention, the particles of the precipitated phosphateserve as the abrasive, and enter between the teeth or between the teethand the gums to physically remove the staining components, together withthe force of brushing. Extrinsic staining materials in teeth have amechanism in which the staining materials are slightly attached to thesurface or the staining materials are attached to the tooth surface bymetals, and therefore, they may be removed by brushing with a toothpastecontaining a chelating agent and an abrasive, and the effect of cleaningthe teeth may be obtained in a short period of time. In addition, ifsmall particles are contained when brushing, they may impart a crunchysensation of use while providing physical stimulation, and therefore,they may leave teeth feeling refreshed after tooth brushing, and mayleave teeth feeling cleaner. Most preferably, the particles have a sizeand strength that may impart a crunchy sensation during tooth brushing.

As used herein, the term “maximum dissolution amount” of phosphaterefers to the amount of phosphate that may be dissolved to the maximumuntil immediately before the supersaturation state of phosphate,depending on the content of used water.

As used herein, the term “excess amount” of phosphate refers to theamount of phosphate that is precipitated to form particles whenphosphate is added in the maximum dissolution amount or more.

The amount of the supersaturated and precipitated phosphate of thepresent invention may be 2% or more, specifically 2% to 10%, morespecifically 3% to 10% or 4% to 9%, and more specifically 5% to 8% or5.5% to 7.5%, based on the total weight of the toothpaste composition,but is not limited thereto.

In particular, when the amount of the supersaturated and precipitatedphosphate is 2% or more based on the total weight of the toothpastecomposition, the crunchy sensation due to particles is realized, and thecleaning power, stain removal power, and whitening effect becomeexcellent. However, when the amount of the supersaturated andprecipitated phosphate exceeds 10% based on the total weight of thetoothpaste composition, it may cause irritation in the mouth.

In the present invention, the solubility of phosphate may be 6 g/100 mLto 100 g/100 mL at 25° C., specifically 20 g/100 mL at 25° C., but isnot limited thereto. The solubility of TSPP is 6.7 g/100 mL (25° C.),the solubility of SAPP is 12.5 g/100 mL (25° C.), and the solubility ofSHMP is 50 g/100 mL (25° C.).

In particular, when the solubility in water is too low, precipitation inthe toothpaste occurs during storage, which is not beneficial to thestability of the composition. In the case of tetrapotassiumpyrophosphate (TKPP) (187 g/100 mL (25° C.)) and potassium acidpyrophosphate (KAPP) (149.25 g/100 mL (25° C.)), the solubility of whichis 100 g/100 mL or more, when 10% phosphate with respect to 10% water isused, it is mostly dissolved, which is not suitable. Pyrophosphate ormetaphosphate has an excellent chelating effect to help the cleaningpower. However, when pyrophosphate or metaphosphate is used in an amountof 10% or more, it may cause irritation in teeth, which is not suitable.

In the present invention, the average diameter of the supersaturated andprecipitated phosphate particles may be 75 μm to 180 μm, specifically105 μm to 180 μm, and more specifically 105 μm to 150 but is not limitedthereto. In particular, when the diameter of the supersaturated andprecipitated phosphate particles is less than 75 it is difficult to feelthe crunchy sensation when the toothpaste composition is used. When thediameter is 75 μm or more, the most excellent crunchy sensation and theexcellent cleaning power are achieved.

In the present invention, the silica refers to silicon dioxide, and thesilica used in the toothpaste agent is prepared by using amorphoussilicon dioxide as a main component. Silica has different properties andabrasiveness depending on a processing method, and may be classifiedinto abrasive silica and thickening silica according to the size ofparticles.

The silica of the present invention may be used in an amount of 15% to50%, specifically 20% to 40%, and more specifically 20% to 30%, based onthe total weight of the toothpaste composition, but is not limitedthereto.

The silica of the present invention may include abrasive silica, and theabrasive silica may be used in an amount of 50% to 90%, specifically 60%to 90%, and more specifically 70% to 90%, based on the total weight ofthe silica, but is not limited thereto.

The toothpaste composition of the present invention, which includes thesilica and the chelating agent containing phosphate, may include water,and the content of water is the same as described above.

In the present invention, phosphate may be supersaturated andprecipitated by reducing the content of water. However, considering thesolubility of phosphate, the content of water may be appropriatelyadjusted.

The toothpaste composition of the present invention, which includes thesilica and the chelating agent containing phosphate, may be used forwhitening and stain removal. According to one exemplary embodiment ofthe present invention, the toothpaste composition of the presentinvention was confirmed to have the effects of improving the cleaningpower and the stain removal power. The toothpaste composition of thepresent invention was confirmed to have the excellent effect of removingstains on the tooth surface and brightening teeth.

According to one exemplary embodiment of the present invention, it wasconfirmed that the toothpaste composition of the present inventionrealized the crunchy sensation to improve sense of use.

The toothpaste composition of the present invention, which includes thesilica and the chelating agent containing phosphate, may further includeone or more components selected from the group consisting of anabrasive, a surfactant, a humectant, a medicinal agent, an additive, anda foaming agent, but is not limited thereto.

In particular, the abrasive, the surfactant, the humectant, themedicinal agent, the additive, and the foaming agent are the same asdescribed above.

According to still another aspect of the present invention, thetoothpaste composition of the present invention includes a peroxide, athickener, and a spreading agent.

Even when the toothpaste composition of the present invention, whichincludes the peroxide, the thickener, and the spreading agent, iscontained in a toothpaste container made of a hydrophobic material suchas PE, phase stability of the toothpaste composition may be maintained.

The toothpaste composition of the present invention provides atoothpaste composition in which the peroxide and the thickener areseparated from each other.

Particularly, even when the peroxide and the thickener are separatedfrom each other in the toothpaste composition, phase stability of thetoothpaste composition may be maintained, and thus activity of thehydrogen peroxide is not deteriorated, and a release rate of thehydrogen peroxide is remarkably high as compared with common toothpastecompositions including a complex of PVP and hydrogen peroxide, therebyachieving a more excellent whitening effect.

As used herein, the term “spreading agent” refers to a material thatimparts hydrophobicity to the toothpaste composition to solve theproblem of separation from polyethylene (PE) in the toothpaste tube andphase separation, thereby improving the phase stability of thetoothpaste composition, and the spreading agent is a safe material forthe human body. The toothpaste composition of the present inventionusing the spreading agent tightly sticks to the material of thetoothpaste tube, so that water generated by hydrolysis does not existbetween the toothpaste and the tube, thereby suppressing phaseseparation, and as a result, stability of the toothpaste is remarkablyimproved.

The spreading agent of the present invention may be one or morecomponents selected from the group consisting of Span 20 (sorbitanmonolaurate), Span 40 (sorbitan monopalmitate), Span 60 (sorbitanmonostearate), Span 80 (sorbitan monooleate), Span 85 (sorbitantrioleate), and TWEEN (POE sorbitan fatty acid ester), and specificallymay be Span 80 (sorbitan monooleate), Span 60 (sorbitan monostearate),or a combination thereof, but is not limited thereto.

The content of the spreading agent of the present invention may be 0.1%by weight to 10% by weight, specifically 0.2% by weight to 5% by weight,and more specifically 0.2% by weight to 2.5% by weight, based on thetotal weight of the toothpaste composition, but is not limited thereto.

As used herein, the term “thickener” is the same as described above.

In the toothpaste composition of the present invention, which includesthe peroxide, the thickener, and the spreading agent, the thickener hasexcellent compatibility with hydrogen peroxide and has a swellingeffect, and thus exhibits the excellent thickening effect even underanhydrous conditions, and exhibits excellent sense of use due to nostickiness.

When the thickener of the present invention forms a complex withhydrogen peroxide, it is known to prevent degradation of hydrogenperoxide by physically separating hydrogen peroxide blended in thetoothpaste composition from other components blended in the toothpastesuch as water, the abrasive, the foaming agent, and the activeingredient of toothpaste, thereby preventing a problem of lowered titerof hydrogen peroxide during distribution of the toothpaste composition.However, since this complex form of thickener—hydrogen peroxide acts asa hindrance factor in exerting the activity of hydrogen peroxide at thetime when a consumer actually uses the toothpaste, it is necessary topretreat or post-treat with a composition containing a separate hydrogenperoxide decomposition agent.

The content of the thickener of the present invention may be 5% byweight to 20% by weight, specifically 7% by weight to 17% by weight, andmore specifically 10% by weight to 15% by weight, based on the totalweight of the toothpaste composition, but is not limited thereto.

The peroxide of the present invention has a tooth whitening effectbecause oxygen generated during peroxide decomposition bleaches stainingmaterials on teeth. Since the peroxide has a relatively low molecularweight, it is effective in achieving high tooth-whitening power at thesame weight.

The peroxide of the present invention may be specifically one or morecomponents selected from the group consisting of hydrogen peroxide,carbamide peroxide, calcium peroxide, sodium percarbonate, sodiumperborate, and tetrasodium pyrophosphate peroxidate, and morespecifically, the peroxide may be hydrogen peroxide, but is not limitedthereto.

The content of the peroxide of the present invention may be 0.1% byweight to 10% by weight, specifically 0.5% by weight to 5% by weight,and more specifically 3% by weight, based on the total weight of thetoothpaste composition, but is not limited thereto.

The toothpaste composition of the present invention may further includean abrasive.

The abrasive is the same as described above.

In one specific embodiment, the toothpaste composition of the presentinvention, which includes the peroxide, the thickener, and the spreadingagent, may include one or more abrasives selected from the groupconsisting of calcium pyrophosphate (CPP), insoluble sodiummetaphosphate, zirconium silicate, and hydroxyapatite, and specifically,the tooth composition may be CPP in terms of stably maintaining activityof peroxide in the toothpaste composition, but is not limited thereto.

Since the peroxide and the abrasive show poor compatibility with eachother, the peroxide and the abrasive are not used together in thetoothpaste composition. However, the toothpaste composition of thepresent invention may include both the peroxide and the abrasive, andtherefore, a synergistic effect may be obtained to achieve an excellentwhitening effect.

The content of the abrasive of the present invention may be 5% by weightto 20% by weight, specifically 7% by weight to 17% by weight, and morespecifically 10% by weight to 15% by weight, based on the total weightof the toothpaste composition, but is not limited thereto.

In one specific embodiment, the toothpaste composition of the presentinvention, which includes the peroxide, the thickener, and the spreadingagent, may include no water, but is not limited thereto.

The toothpaste composition of the present invention may be used fortooth whitening.

Specifically, the toothpaste composition of the present invention, whichincludes the peroxide, the thickener, and the spreading agent, and inwhich the peroxide and the thickener are separated from each other, mayexhibit a much more excellent tooth whitening effect due to remarkablyrapid decomposition of hydrogen peroxide when actually used, as comparedwith common toothpaste compositions including the thickener and hydrogenperoxide in the complex form.

The toothpaste composition of the present invention may have improvedphase stability even at 30° C. to 60° C., and specifically, no phaseseparation phenomenon of the peroxide occurs even after 4 weeks. Thetoothpaste composition tightly sticks to the tube, so that watergenerated by hydrolysis does not exist, thereby suppressing the phaseseparation phenomenon. Therefore, even in the toothpaste composition ofthe present invention, which includes the peroxide, the thickener, andthe spreading agent, and in which the peroxide and the thickener areseparated from each other, stability of the toothpaste may be remarkablyimproved.

The toothpaste composition of the present invention, which includes theperoxide, the thickener, and the spreading agent, may further includeone or more components selected from the group consisting of asurfactant, a humectant, a medicinal agent, an additive, and a foamingagent, but is not limited thereto.

The abrasive, the surfactant, the humectant, the medicinal agent, theadditive, and the foaming agent are the same as described above.

MODE FOR CARRYING OUT THE INVENTION

Hereinafter, the present invention will be described in more detail withreference to the following Examples. However, the following Examples arefor illustrative purposes only, and the scope of the present inventionis not intended to be limited by these Examples.

Examples 1 to 4 and Comparative Examples 1 to 4

Toothpaste compositions of Examples 1 to 4 and Comparative Examples 1 to4 were prepared according to components and composition ratios shown inTable 1 below.

Specifically, a structurant (carrageenan or carbomer) and a thickener(poloxamer or xanthan gum) were dispersed in a humectant (PEG, glycerin,etc.) in advance, and salt components (sodium fluoride, saccharin, etc.)dissolved or dispersed in purified water were added thereto, followed byhydration under stirring. Silica (abrasive silica or thickening silica)was mixed therewith by dispersion, followed by stirring for 20 minutes.Thereafter, a foaming agent (SLS, etc.) was added thereto, followed bystirring under vacuum for 20 minutes. A flavor was added thereto,followed by stirring under vacuum for 20 minutes, and thereby eachtoothpaste composition was prepared. However, the toothpastecompositions of the present invention are not limited to the abovepreparation method.

TABLE 1 Comparative Comparative Comparative Comparative Example 1Example 2 Example 3 Example 4 Example 1 Example 2 Example 3 Example 4Glycerin 56.05 54.95 58.55 54.2 38.75 45.15 54.55 45.55 Abrasive 20 1515 20 5 15 25 22 silica Thickening 2 10 7 5 9 0 0 0 silica STPP 4 4 8 44 (sodium tripolyphosphate) SHMP 8 (sodium hexametaphosphate) TSPP 4 4(tetrasodium pyrophosphate) Purified 10 8 7 5 30 27 8 20 water PEG 3 3 33 3 3 3 3 Flavor 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 Triphosphate 1.0 1.01.0 1.0 1.0 1.0 1.0 1.0 SLS 2.0 2.0 2.0 2.0 2.0 2.0 2.0 2.0 (sodiumlauryl sulfate) Carrageenan 0.4 0.2 0.15 0.2 Carbomer 0.5 0.5 Poloxamer0.4 0.4 CMC 1.5 0.45 Xanthan gum 0.1 0.5 0.3 0.1 0.75 0.4 0.5 Saccharin0.15 0.2 0.2 Titanium 0.23 0.23 0.23 0.23 0.23 0.23 0.23 0.23 oxideSodium 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 fluoride

Experimental Example 1. Measurement of Physical Properties ofToothpastes

(1) Method of Measuring Viscosity

Viscosity was measured using a viscometer (Brookfield RVF) and a spindlebar of #7 at a rotational speed of 20 rpm (Spindle bar) at 25° C.

(2) Method of Measuring Suitability for Tube

It was evaluated whether each of the toothpaste compositions could beinjected into a common toothpaste tube.

(3) Method of Measuring Release Property

1) Method of Measuring Consumers' Evaluation of Release Property

Slurries were directly prepared and stirred for a predetermined time,and then consumers directly evaluated the degree of the releaseproperty. 12 adults were allowed to brush their teeth using each of thetoothpastes of Examples 1 to 4 and Comparative Examples 1 to 4 in alength of 1 cm, and to evaluate the release property with a 5-pointscale: 5 points given for very good, 4 points for good, 3 points formoderate, 2 points for slightly poor, and 1 point for very poor.

2) Method of Measuring Release Property Using Laboratory Beakers

12.5 g of each toothpaste was put in a 50 mL beaker, and 20 g of waterwas added thereto, followed by vigorous stirring for 30 seconds using aglass rod. The toothpaste slurry in the beaker was transferred to astainless plate, and then the remaining amount and shape thereof werevisually examined, and rated as follows: 5 points given for nothing leftafter being completely dissolved, 4 points for a small amount left butmostly dissolved, 3 points for no large lumps left after being fairlydissolved, 2 points for a considerable amount of undissolved lumps, and1 point for large lumps not dissolved but clumped together.

(4) Method of Measuring Phase Angle

Phase angle (δ) was measured by measuring G″/G′, a loss tangent (tan δ)value, with respect to the toothpaste compositions of Examples 1 to 4and Comparative Examples 1 to 4 using a rheometer.

(5) Method of Measuring Low-Shear Viscosity

Shear viscosity was measured with respect to the toothpaste compositionsof Examples 1 to 4 and Comparative Examples 1 to 4 at a shear rate of0.1 s⁻¹.

(6) Results of Measuring Physical Properties

The results of measuring the viscosity, release property (consumers'evaluation, laboratory evaluation), phase angle, and low-shear viscositywith respect to the toothpaste compositions of Examples 1 to 4 andComparative Examples 1 to 4 are shown in Table 2 below.

TABLE 2 Comparative Comparative Comparative Comparative Example 1Example 2 Example 3 Example 4 Example 1 Example 2 Example 3 Example 4Viscosity 70,000 80,000 50,000 100,000 110,000 20,000 40,000 25,000 Tubesuitability Pass Pass Pass Pass Pass Fail Fail Fail Releasing property 54 4 5 2.5 4 4 3 (consumers' evaluation scale) Releasing property 4 4 4 51 4 4 2 (laboratory evaluation) Phase angle 32 35 37 30 11.1 27.4 35 8.2Low-shear 858,000 566,000 388,000 797,000 8,135,000 413,000 699,0001,530,000 viscosity (cP)

From the results of Table 2, it was confirmed that all toothpastecompositions of Examples 1 to 4 according to the present invention weregiven very excellent ratings with regard to the release property(consumers' evaluation and laboratory evaluation) even at a viscosity of50,000 or more, as compared with the toothpaste compositions ofComparative Examples 1 to 4, and showed excellent suitability fortoothpaste tubes and phase angle of 25 or more.

Experimental Example 2. Measurement of Sense of Use

(1) Method of Measuring Feeling of Refreshment and Flavor ReleasingPower

12 adults were allowed to brush their teeth using the same toothbrush(Reach Sensitive Toothbrush) and each of the toothpaste compositions ofExamples 1 to 4 and Comparative Examples 1 to 4 in a length of 1 cm for1 minute, and then the flavor releasing power and the feeling ofcleaning were surveyed.

Survey Response Criteria

5: A feeling of refreshment and a flavor releasing power are obviouslybetter than those of toothpastes used before.

4: A feeling of refreshment and a flavor releasing power are slightlybetter than those of toothpastes used before.

3: A feeling of refreshment and a flavor releasing power are similar tothose of toothpastes used before.

2: A feeling of refreshment and a flavor releasing power are slightlyworse than those of toothpastes used before.

1: A feeling of refreshment and a flavor releasing power are obviouslyworse than those of toothpastes used before.

(2) Method of Measuring Stain Removal Effect/Cleaning Effect

20 adult males who are daily smokers were allowed to brush their teethusing the same toothbrush (Reach Sensitive Toothbrush) and each of thetoothpaste compositions of Examples 1 to 4 and Comparative Examples 1 to4 in a length of 1 cm for 1 minute three times a day for 4 weeks, andthen the cleaning power was surveyed.

Survey Response Criteria

5: You feel like stains on the tooth surface are removed and the teethare brightened.

4: You feel like stains on the tooth surface are slightly removed.

3: You feel like the teeth are slightly brightened.

2: You feel like the tooth surface becomes smooth.

1: You feel like there is no great difference before and after use.

(3) Results of Measuring Sense of Use

The results of measuring the feeling of refreshment, flavor releasingpower, and stain removal effect/cleaning effect with respect to thetoothpaste compositions of Examples 1 to 4 and Comparative Examples 1 to4 are shown in Table 3 below.

TABLE 3 Comparative Comparative Comparative Comparative Example 1Example 2 Example 3 Example 4 Example 1 Example 2 Example 3 Example 4Feeling of 4 5 5 5 3 4 2 1 Refreshment, Flavor releasing power Stain 4 54 5 3 3 3 3 removal, Cleaning effect

From the results of Table 3, it was confirmed that, as compared with thetoothpaste compositions of Comparative Examples 1 to 4, all toothpastecompositions of Examples 1 to 4 according to the present inventionobviously showed a more excellent feeling of refreshment and flavorreleasing power than toothpastes used before, and showed an excellentstain removal effect and cleaning effect, as it was evaluated that thestains on the tooth surface seemed to be removed and the teeth seemed tobe brightened.

Preparation of Examples 5 to 9 and Comparative Examples 5 to 9

Toothpaste compositions of Examples 5 to 9 and Comparative Examples 5 to9 were prepared according to components and composition ratios shown inTable 4 below. Specifically, other components (additive, etc.) dissolvedin purified water were mixed with a thickener (carrageenan or xanthangum) that had been dispersed in a humectant (PEG or glycerin), and thensilica (abrasive or thickening silica) was added thereto, followed bystirring for about 20 minutes. A surfactant (SLS, etc.) was addedthereto, followed by stirring under vacuum for about 20 minutes. Achelating agent (SHMP, TSPP, or SAPP) and a flavor were added thereto,followed by stirring under vacuum for about 20 minutes, and thereby eachtoothpaste was prepared.

The viscosity of each toothpaste composition was measured using aviscometer (Brookfield RVF) and a spindle bar of #7 at a rotationalspeed of 20 rpm at 25° C. for 5 rotations (15 seconds), and the resultsare shown in Table 4 below.

TABLE 4 Comparative Comparative Comparative Comparative ComparativeExample 5 Example 6 Example 7 Example 8 Example 9 Example 5 Example 6Example 7 Example 8 Example 9 Water 2.72 4.00 5.00 5.00 5.00 16.95 18.9512.00 13.00 16.00 Microbeads 2.00 TSPP 5.68 SAPP 6.00 >75 μm 8.00 8.008.00 8.00 SHMP 105-180 μm 8.00 10.00 SHMP Sodium 1.00 1.00 1.00 1.001.00 1.00 1.00 1.00 1.00 1.00 phosphate tribasic Abrasive 20.00 20.0020.00 20.00 20.00 20.00 20.00 20.00 20.00 20.00 silica Thickening 5.005.00 5.00 5.00 5.00 9.00 9.00 3.00 3.00 5.00 silica Glycerin 58.60 57.0054.00 54.00 52.00 43.00 43.00 48.15 47.15 41.95 PEG 3.00 3.00 3.00 3.003.00 3.00 3.00 3.00 3.00 3.00 (polyethylene glycol) Carrageenan 0.150.15 0.15 0.15 0.15 1.20 1.20 0.80 0.80 1.20 Xanthan 0.30 0.30 0.30 0.300.30 0.30 0.30 0.50 0.50 0.30 gum SLS 2.00 2.00 2.00 2.00 2.00 2.00 2.002.00 2.00 2.00 (sodium lauryl sulfate) Titanium 0.23 0.23 0.23 0.23 0.230.23 0.23 0.23 0.23 0.23 oxide Sodium 0.10 0.10 0.10 0.10 0.10 0.10 0.100.10 0.10 0.10 saccharin Flavor 1.00 1.00 1.00 1.00 1.00 1.00 1.00 1.001.00 1.00 Sodium 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22 0.22fluoride Maximum 0.18 0.50 2.50 2.50 2.50 — — 6.00 6.50 8.00 dissolutionamount Supersaturation 5.50 5.50 5.50 5.50 7.50 — — 2.00 1.50 0.00(excess amount) Viscosity 85,000 80,000 75,000 76,000 78,000 85,00080,000 76,000 74,000 85,000 (cP)

Experimental Example 3. Measurement of In Vitro Cleaning Effect andWhitening Effect

(1) Method of Measuring In Vitro Cleaning Effect and Whitening Effect

Artificial teeth (tooth enamel, hydroxyapatite, which is a materialprimarily constituting dentin) were prepared into tablet specimens, andstained using tooth staining materials such as tea, coffee, mucin, metalsalts, etc. Thereafter, the hydroxyapatite tablet specimens were fixedusing a brushing machine for testing cleaning power. The toothpastecomposition of the present invention was brushed in a slurry state atthe actual concentration (25 g/40 mL) 5400 times at a speed of 90 timesper second, and the degree of brightness of the stained artificial toothspecimen before and after cleaning was determined by measuring a colorchange (ΔE) in the surface of hydroxyapatite tablet specimen using achromameter.

(2) Results of Measuring In Vitro Cleaning Effect and Whitening Effect

The results of measuring an in vitro tooth whitening effect with respectto the toothpaste compositions of Examples 5 to 9 and ComparativeExamples 5 to 9 are shown in Table 5 below.

TABLE 5 Comparative Comparative Comparative Comparative ComparativeExample 5 Example 6 Example 7 Example 8 Example 9 Example 5 Example 6Example 7 Example 8 Example 9 Δ E 16.1 16.7 18.5 20.1 22.5 9.0 8.0 14.614.5 14.0

From the results of Table 5, it was confirmed that the toothpastecompositions of Examples 7 to 9 using SHMP as phosphate showed awhitening effect 2.1 to 2.8 times higher than that of the toothpastecompositions of Comparative Examples 5 and 6 without SHMP as phosphate,and also showed a whitening effect 1.3 to 1.6 times higher than that ofthe toothpaste compositions of Comparative Examples 7 to 9 using SHMP asphosphate and water in an amount of 10% or more, based on the totalweight of the toothpaste composition.

In addition, it was confirmed that the toothpaste compositions ofExample 5 and 6 each using TSPP or SAPP as phosphate showed a whiteningeffect 1.8 to 2.1 times higher than that of the toothpaste compositionsof Comparative Examples 5 and 6 using no SHMP as phosphate.

These results suggest that the toothpaste compositions having more than2% of phosphate supersaturation based on the total weight of thetoothpaste composition, by including SHMP and 10% or less of water basedon the total weight of the toothpaste composition, provide a feeling ofparticles to effectively remove staining materials on the tooth surface,thereby exhibiting a more excellent tooth whitening effect.

Experimental Example 4. Measurement of Sense of Use

(1) Method of Measuring Crunchy Sensation

12 adults were allowed to brush their teeth using the same toothbrush(Reach Sensitive Toothbrush) and each of the toothpaste compositions ofExamples 5 to 9 and Comparative Examples 5 to 9 in a length of 1 cm for1 minute three times a day for 2 weeks, and then the crunchy sensationwas surveyed.

Survey Response Criteria

5: You feel like a crunchy sensation is obviously better than that oftoothpastes used before.

4: You feel like a crunchy sensation is slightly better than that oftoothpastes used before.

3: You feel particles in the toothpaste.

2: You feel like a crunchy sensation is similar to that of toothpastesused before.

1: You feel like a crunchy sensation is obviously worse than that oftoothpastes used before.

(2) Method of Measuring Feeling of Cleaning

12 adults were allowed to brush their teeth using the same toothbrush(Reach Sensitive Toothbrush) and each of the toothpaste compositions ofExamples 5 to 9 and Comparative Examples 5 to 9 in a length of 1 cm for1 minute three times a day for 2 weeks, and then the feeling of cleaningwas surveyed.

Survey Response Criteria

5: After brushing teeth, you feel the tooth surface is clean and feel asqueaky sound.

4: After brushing teeth, you feel the tooth surface is clean.

3: After brushing teeth, you feel a squeaky sound.

2: You feel like there is no great difference in cleaning power comparedto toothpastes used before.

1: You feel like the cleaning power is worse than that of toothpastesused before.

(3) Results of Measuring Sense of Use

The results of measuring the crunchy sensation and the feeling ofcleaning with respect to the toothpaste compositions of Examples 5 to 9and Comparative Examples 5 to 9 are shown in Table 6 below.

TABLE 6 Comparative Comparative Comparative Comparative ComparativeExample 5 Example 6 Example 7 Example 8 Example 9 Example 5 Example 6Example 7 Example 8 Example 9 Crunchy 3.5 3.5 4 4.5 5 3 2 2.5 2.5 2sensation Feeling of 4 4 4 4.5 5 2 2 3 3 3 cleaning

From the results of Table 6, it was confirmed that, as compared with thetoothpaste compositions of Comparative Examples 5 to 9, all toothpastecompositions of Example 5 to 9 according to the present invention showeda much more excellent crunchy sensation than toothpastes used before,and showed the excellent feeling of cleaning, as it was evaluated thatthe tooth surface seemed to be clean and a squeaky sound could be felt.

Preparation of Examples 10 to 17

Toothpaste compositions of Examples 10 to 17 were prepared according tocomponents and composition ratios shown in Table 7 below.

Specifically, all liquid components were added to a humectant (PG, PEG,glycerin), followed by mixing well. Then, an abrasive (CPP, silica) anda thickener (PVP or crossed linked PVP) were well dispersed. Othercomponents (additive, etc.) were dispersed therein, followed by stirringfor about 20 minutes. A surfactant (SLS, etc.) was added thereto,followed by stirring under vacuum for about 20 minutes. Hydrogenperoxide and a flavor were added thereto, followed by stirring undervacuum for about 20 minutes, and thereby each toothpaste was prepared.The preparation method of the present invention is not limited thereto.

TABLE 7 Example 10 Example 11 Example 12 Example 13 Example 14 Example15 Example 16 Example 17 PG 32.3 33.3 32.8 41.88 42.88 42.38 34.8 34.8PEG 10 10 10 10.2 10.2 10.2 10 10 Glycerin 10 10 10 2.5 2.5 2.5 10 10EO-PO block 10 10 10 11.4 11.4 11.4 10 10 copolymer NaF 0 0 0 0.21 0.210.21 0 0 SMFP 0.68 0.68 0.68 0.68 0.68 TSPP 1.5 1.5 1.5 1.0 1.0 1.0 1.51.5 SAPP 0.5 0.5 0.5 1.0 1.0 1.0 0.5 0.5 Silica 2 2 2 3.0 3.0 3.0 2 2CPP 15 15 15 10 10 10 15 15 Sorbitan 2 0 0.5 2 0 0.5 2 2 monooleateSorbitan 0 1 0 0 1 0 0 0 monostearate Polysorbate 80 0 0 1.0 0 0 1.0 0 0PVP 0 0 0 5.5 Crosslinke 10.5 10.5 10.5 11.0 11.0 11.0 5.5 0 dPVPPVP-H₂O₂ 0 0 0 0 0 0 0 5.5 complex (H₂O₂ 19%) Crosslinked 0 0 0 0 0 05.5 0 PVP-H₂O₂ complex (H₂O₂ 19%) H₂O₂ (35%) 3.0 3.0 3.0 3.0 3.0 3.0 0 0SLS 2.0 2.0 2.0 2 2 2 2 2.0 Sodium 0.5 0.5 0.5 0.8 0.8 0.8 0.5 0.5saccharin Sucralose 0.02 0.02 0.02 0.01 0.01 0.01 0.02 0.02 Water 0 0 00 0 0 0 0

Preparation of Comparative Examples 10 to 15

Toothpaste compositions of Comparative Examples 10 to 14 were preparedaccording to components and composition ratios shown in Table 8 below inthe same manner as in Examples 10 to 17, except for whether hydrogenperoxide was used or not, whether CPP (calcium pyrophosphate) was usedor not, and that a thickener (crosslinked PVP—H₂O₂ complex) and aspreading agent were not used. A commercially available MEDIAN dentalwhitening toothpaste (containing hydrogen peroxide, containing noabrasive, and containing water) was used as Comparative Example 15.

TABLE 8 Comparative Comparative Comparative Comparative ComparativeExample 10 Example 11 Example 12 Example 13 Example 14 PG 34.3 36.8134.31 51.81 37.3 PEG 10 10 10 10 10 Glycerin 10 10 10 10 10 EO-PO 10 1010 10 10 block copolymer NaF 0 0 0 0 0 SMFP 0.68 0.68 0.68 0.68 0.68TSPP 1.5 1.5 1.5 1.5 1.5 SAPP 0.5 0.5 0.5 0.5 0.5 Silica 2 2 2 2 2 CPP15 15 15 0 15 Sorbitan 0 0 0 0 0 monooleate Sorbitan 0 0 0 0 0monostearate Polysorbate 0 0 0 0 0 80 PVP 0 0 10.5 0 0 Crosslinked 10.55.5 0 5.5 10.5 PVP PVP-H₂O₂ 0 0 0 0 0 complex Crosslinked 0 5.5 0 5.5 0PVP-H₂O₂ complex H₂O₂ (35%) 3.0 0 3.0 0 0 SLS 2.0 2 2 2 2.0 Sodium 0.50.5 0.5 0.5 0.5 saccharin Sucralose 0.02 0.01 0.01 0.01 0.02 Water 0 0 00 0

Experimental Example 5. Measurement of Stability of Toothpaste

(1) Method of Measuring Stability of Hydrogen Peroxide at HighTemperature Over Time

According to a titration method of using iodine, which is a method ofindirectly measuring a hydrogen peroxide concentration, the hydrogenperoxide concentrations early after preparation of the toothpaste andafter storing the toothpaste in the tube for 4 weeks in a 50° C. waterbath were measured, and a ratio of the concentration of remaininghydrogen peroxide to the initial concentration of hydrogen peroxide wascalculated. When no decomposition occurred, it was expressed as 100%.

(2) Method of Measuring Phase Stability of Toothpaste at HighTemperature

After storing the toothpaste in the tube for 4 weeks in a 50° C. waterbath, the surface condition was visually observed to examine whetherthere was any liquid separation when the toothpaste was squeezed, andwhether the content of the toothpaste tightly stuck in the tube when thetube was cut in half.

(3) Results of Measuring Stability of Toothpaste

The results of measuring stability of hydrogen peroxide at a hightemperature over time and phase stability of the toothpaste at a hightemperature with respect to the toothpaste compositions of Examples 10to 12, 16, and 17 and Comparative Examples 10 to 14 are shown in Table 9below.

TABLE 9 Compar- Compar- Compar- Compar- Compar- ative ative ative ativeative Stored at Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam- Exam-Exam- 50° C. ple 10 ple 11 ple 12 ple 16 ple 17 ple 10 ple 11 ple 12 ple13 ple 14 Residual 90% 91% 90% 91% 90% 86% 88% 88% 86% Not peroxideadded ratio (%) after 4 weeks Toothpaste 5 5 5 4 4 3 1 2 2 3 phasestability in tube after 4 weeks

From the results of Table 9, it was confirmed that 90% or more of theperoxide of the toothpaste compositions of Examples 10 to 12, 16, and 17was not decomposed even after 4 weeks, and the toothpaste compositionsof Examples 10 to 12, and 16 were not separated from the tube andtightly stuck in the tube even after 4 weeks, unlike the toothpastecompositions of Comparative Examples 10 to 14 which were separated fromthe tube after 4 weeks (FIG. 3 ), indicating that due to use of thespreading agent, the toothpaste compositions tightly stuck in the tube,and thus water generation due to hydrolysis did not occur to inhibit aphase separation phenomenon, and as a result, the toothpaste compositionincluding hydrogen peroxide and the thickener, in which hydrogenperoxide and the thickener are separated from each other, may haveremarkably improved stability of the toothpaste.

Experimental Example 6. Measurement of Sense of Use and Whitening Effectof Toothpaste

(1) Method of Measuring Feelings of Refreshment and Cleaning

10 adults were allowed to brush their teeth using the toothpastecompositions of Examples 10 to 17 and Comparative Examples 10 to 15 for1 minute or more three times a day for 1 month, and then the feelings ofrefreshment and cleaning were surveyed.

Survey Response Criteria

5: Feelings of refreshment and cleaning are given, like those oftoothpastes used before.

4: Both feelings of cleaning and refreshment after use are acceptable.

3: Any one feeling of cleaning and refreshment after use is acceptable.

2: Both feelings of cleaning and refreshment after use areunsatisfactory, even though you do not want to use another toothpaste.

1: Both feelings of cleaning and refreshment after use are veryunsatisfactory such that you want to use another toothpaste.

(2) Method of Measuring Stickiness

10 adults were allowed to brush their teeth using the toothpastecompositions of Examples 10 to 17 and Comparative Examples 10 to 15 for1 minute or more three times a day for 1 month, and then the stickinesswas surveyed.

Survey Response Criteria

5: It is not sticky.

4: It is a little sticky, but there is no problem in using it.

3: It is very sticky, but there is no problem in using it.

2: It is too sticky to brush your teeth.

1: It is so sticky that it is uncomfortable to squeeze it on thetoothbrush.

(3) Method of Measuring Whitening Effect and Cleaning Power

10 adults were allowed to brush their teeth using the toothpastecompositions of Examples 10 to 17 and Comparative Examples 10 to 15 for1 minute or more three times a day for 1 month, and then the whiteningeffect and cleaning power were surveyed.

Survey Response Criteria

5: You feel like the teeth are obviously brightened.

4: You feel like the tooth surface becomes smooth and the teeth arebrightened.

3: You feel like the teeth are slightly brightened.

2: You feel like the tooth surface becomes a little clean.

1: You feel no difference in the whitening effect and the feeling ofcleaning before and after use.

(4) Method of Measuring In Vitro Tooth Whitening Effect

Artificial teeth (tooth enamel, hydroxyapatite, which is a materialprimarily constituting dentin) were prepared into tablet specimens, andstained using tooth staining materials such as tea, coffee, mucin, metalsalts, etc. Thereafter, the toothpaste was brushed in a slurry state atthe actual concentration (25 g/40 mL) 5,400 times at a speed of 90 timesper second by using a brushing machine for testing a cleaning power, andthe degree of brightness of the stained artificial tooth specimen beforeand after cleaning was measured using a chromameter, and a color change(ΔE) was calculated.

(5) Results of measuring sense of use and whitening effect

1) Results of Measuring Sense of Use

The results of measuring the in vitro tooth whitening effect withrespect to the toothpaste compositions of Examples 10 to 17 andComparative Examples 10 to 15 are shown in Table 10 below.

TABLE 10 Example 10 Example 11 Example 12 Example 13 Example 14 Example15 Example 16 Feeling of 5 5 5 5 5 5 5 refreshment and cleaningStickiness 5 5 5 5 5 5 5 Whitening 5 5 5 5 5 5 4 effect and Cleaningpower Comparative Comparative Comparative Comparative ComparativeComparative Example 17 Example 10 Example 11 Example 12 Example 13Example 14 Example 15 Feeling of 2 4 4 2 2 1 1 refreshment and cleaningStickiness 1 5 5 1 4 5 5 Whitening 4 4 4 4 3 2 3 effect and Cleaningpower

From the results of Table 10, it was confirmed that the toothpastecompositions of Examples 10 to 17 provided excellent feelings ofcleaning and refreshment, no stickiness, and an excellent whiteningeffect by remarkably brightening the teeth, as compared with ComparativeExamples 10 to 15, indicating that due to the use of crosslinked PVP asthe thickener, the toothpaste compositions have no stickiness andimproved sense of use.

2) Results of Measuring In Vitro Tooth Whitening Effect

The results of measuring the in vitro tooth whitening effect withrespect to the toothpaste compositions of Examples 10 to 12, 16, and 17and Comparative Examples 11, 13, and 14 are shown in Table 11 below.

TABLE 11 Comparative Comparative Comparative Comparative Example 10Example 11 Example 12 Example 16 Example 17 Example 10 Example 11Example 13 Example 14 ΔE 26.8 ± 25.9 ± 26.3 ± 21.5 ± 20.8 ± 26.0 ± 20.9± 11.5 ± 14.0 ± (5400 0.44 0.71 0.90 0.57 0.29 1.02 0.25 0.85 1.20times)

From the results of Table 11, it was confirmed that the toothpastecompositions of Examples 10 to 12, 16, and 17, in which hydrogenperoxide and the thickener are separated from each other, exhibited awhitening effect 1.3 to 2.3 times higher than that of the toothpastecompositions of Comparative Examples 11, 13, and 14, in which a complexof hydrogen peroxide and the thickener is included, indicating that thetoothpaste compositions including hydrogen peroxide and the thickener,in which hydrogen peroxide and the thickener are separated from eachother, may exhibit a much more excellent whitening effect due toremarkably rapid decomposition of hydrogen peroxide when actually used.

Based on the above description, it will be understood by those skilledin the art that the present invention may be implemented in a differentspecific form without changing the technical spirit or essentialcharacteristics thereof. Therefore, it should be understood that theabove embodiment is not limitative, but illustrative in all aspects. Thescope of the present invention is defined by the appended claims ratherthan by the description preceding them, and therefore all changes andmodifications that fall within metes and bounds of the claims, orequivalents of such metes and bounds are therefore intended to beembraced by the claims.

1. A toothpaste composition comprising a structurant and a thickener. 2.The toothpaste composition of claim 1, wherein the toothpastecomposition has a phase angle of 20 to
 90. 3. The toothpaste compositionof claim 1, wherein the toothpaste composition has viscosity of 50,000cP to 120,000 cP after being stored for 7 days at 20° C. to 30° C. 4.The toothpaste composition of claim 1, wherein the structurant is one ormore components selected from the group consisting of carrageenan andcarbomer.
 5. The toothpaste composition of claim 1, further comprisingwater in an amount of 1% by weight to 15% by weight.
 6. The toothpastecomposition of claim 1, wherein the thickener comprises an organicthickener and an inorganic thickener.
 7. The toothpaste composition ofclaim 6, wherein the organic thickener comprises no carboxymethylcellulose (CMC), and is one or more components selected from the groupconsisting of poloxamer, carbomer, and polysaccharide.
 8. The toothpastecomposition of claim 7, wherein the polysaccharide is one or morecomponents selected from the group consisting of xanthan gum, gellangum, and locust bean gum.
 9. The toothpaste composition of claim 6,wherein the inorganic thickener is one or more components selected fromthe group consisting of thickening silica, colloidal silica, and fumedsilica.